CN106242550A - A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof - Google Patents
A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof Download PDFInfo
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- CN106242550A CN106242550A CN201610584792.0A CN201610584792A CN106242550A CN 106242550 A CN106242550 A CN 106242550A CN 201610584792 A CN201610584792 A CN 201610584792A CN 106242550 A CN106242550 A CN 106242550A
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- C04B35/803—
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/447—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on phosphates, e.g. hydroxyapatite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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Abstract
A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof, step is: configuration aluminum phosphate solution: aluminium salt being incorporated in phosphate aqueous solution, arranging bath temperature is 60～100 DEG C, it is thus achieved that transparent aluminium dihydrogen phosphate aqueous solution；Configuration is containing one or both silicon nitrides, boron nitride, aluminium oxide or the ceramic slurry of silicon oxide, with ethanol or methanol as solvent, with fluorine containing silane as dispersant；The aluminium dihydrogen phosphate aqueous solution of acquisition is joined in ceramic slurry, continue ball milling and obtain ceramic particle/aluminum phosphate composite ceramics slip, use vibration moulding, ceramic particle/aluminum phosphate composite ceramics the slip making acquisition is sufficiently impregnated with quartz fiber cloth, the fiber cloth obtained successively is stacked, and use compression molding, wherein molding pressure is 2～10MPa, it is thus achieved that composite impregnant；Composite impregnant is placed in drying baker and carries out cured, solidification temperature 80～200 DEG C, hardening time 12～72h, obtain moistureproof wave transparent quartz fibre/phosphate ceramics composite.
Description
Technical field
The present invention relates to a kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof, belong to pottery multiple
Condensation material preparation method technical field.
Background technology
Phosphate polymer material has the rheological behavior of low, the similar resin liquid of preparation temperature, low-density simultaneously
(1.8～2.8g/cm3), higher mechanical strength, extremely low thermal coefficient of expansion (2～6 × 10～6/ K), higher heat resisting temperature with
And the feature such as good structure designability and high-temperature oxidation resistant, the requirement of multiple specific function can be met, be widely used in each
Plant the aerospace craft antenna house such as rocket, guided missile, be also to prepare high performance composites (FRP) comparatively ideal matrix material
Material.It is 170 DEG C that the quartz fibre such as developed strengthens chrome-alumina phosphate composite curing molding temperature, and using temperature is 1200
DEG C, bending strength, up to 120MPa, can be used as missile-borne radome；The aluminum phosphate material of the high-temperature amorphous of recent development
(CerablakTM), the low (2.1g/cm of its density3), thermal conductivity low (1～1.5W/mK), use temperature be up to 1400 DEG C, meet under
The demand of generation hypersonic vehicle；The silicon carbide fibre developed strengthens aluminium phosphate composite, can realize height at X-band
Effect wave-absorbing effect, density is low simultaneously, and density is only 1.83～2.05g/cm3, bending strength is up to 271MPa.As can be seen here, phosphorus
Silicate polymer provides a new way for preparation low-density, fibrous composite corrosion-resistant, high performance.Phosphate is polymerized
The greatest problem run in thing composite application process is the high and high hygroscopic properties of its dielectric constant, and this has a strong impact on compound
The resting period of material and military service stability, need it is carried out low dielectric and damp-proof treatment.But, due to this based material
Application sensitivity and confidentiality are higher, and correlation processing technique does not have been reported that.
Summary of the invention
The invention aims to solve the problem that above-mentioned prior art exists, i.e. phosphate polymer composite should
The greatest problem run into during with is the high and high hygroscopic properties of its dielectric constant, and what this had a strong impact on composite deposits week
Phase and military service stability, need it is carried out low dielectric and damp-proof treatment.And then a kind of moistureproof wave transparent quartz fibre/phosphorus is provided
Hydrochlorate ceramic composite preparation method.
It is an object of the invention to be achieved through the following technical solutions:
A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof, the steps include:
Step 1, configuration aluminum phosphate solution: aluminium salt being incorporated in phosphate aqueous solution, arranging bath temperature is 60～100
DEG C, promote the dissolving of aluminium salt, and obtain transparent aluminium dihydrogen phosphate aqueous solution, in aluminium dihydrogen phosphate aqueous solution, aluminium dihydrogen phosphate
Mass fraction is 40～80wt.%；
Step 2, configuration are containing one or both silicon nitrides, boron nitride, aluminium oxide or the ceramic particle slip of silicon oxide, with second
Alcohol or methanol are solvent, with fluorine containing silane as dispersant；Wherein fluorine containing silane is PFTS (C8F13H4SiCl3)、PFOTES
(C14H19F13O3Si), FAS (C8F13H4Si (OCH2CH3) 3) or PTES (C14H19F15O3Si2) therein one or several
Mixing, in ceramic particle slip, the content of silicon fluoride is 0.1～20wt.%；
Step 3, aluminium dihydrogen phosphate aqueous solution step 1 obtained join in the ceramic particle slip obtained in step 2,
Continue ball milling and obtain ceramic particle/aluminum phosphate composite ceramics slip, in described ceramic particle/aluminum phosphate composite ceramics slip, phosphorus
The mass fraction of acid aluminum is 20～40wt%, and ceramic particle content is 20～50wt%；
Step 4, employing vibration moulding, the ceramic particle/aluminum phosphate composite ceramics slip making step 3 obtain is sufficiently impregnated with stone
English fiber cloth, wherein vibration amplitude 2～5mm, frequency 5～100Hz, time of vibration 1～10min；
Step 5, fiber cloth step 4 obtained successively stack, and use compression molding, wherein molding pressure be 2～
10MPa, it is thus achieved that composite impregnant；
Step 6, composite impregnant step 5 obtained are placed in drying baker and carry out cured, solidification temperature 80
～200 DEG C, hardening time 12～72h, obtain moistureproof wave transparent quartz fibre/phosphate ceramics composite.
Described aluminium salt is aluminium hydroxide, aluminum nitrate.
In described step 1, bath temperature is 85 DEG C.
In described step 4, vibration amplitude 3mm, frequency 56Hz, time of vibration 5min.
In described step 5, molding pressure is 4MPa.
In described step 6, solidification temperature 120 DEG C, 36h hardening time.
Understanding after tested, the phosphate ceramics composite dielectric constant obtained through above-mentioned steps is 2～5 and water
Contact angle ＞ 140 °, i.e. obtains moistureproof wave transparent quartz fibre/phosphate ceramics composite.
The method of the present invention is the problem of high hygroscopic properties during solving phosphate polymer materials application, extends phosphorus
The resting period of silicate composite material, enhances the military service stability of phosphate composite material, have that method is simple, low cost,
Moisture effect is good, suitability advantage widely, can carry out industrialized production on a large scale, can be used for the neck such as Aeronautics and Astronautics and national defence
Territory.
Detailed description of the invention
The present invention is described in further detail below: the present embodiment enters under premised on technical solution of the present invention
Row is implemented, and gives detailed embodiment, but protection scope of the present invention is not limited to following embodiment.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof involved by the present embodiment, by following step
Rapid realization:
Step 1, configuration aluminum phosphate solution: being dissolved in phosphate aqueous solution by aluminium hydroxide, arranging water bath is 70 DEG C,
Obtaining transparent aluminium dihydrogen phosphate aqueous solution, aluminium dihydrogen phosphate mass fraction is 50wt.%；
Step 2, configuration boron nitride ceramics slip, with ethanol as solvent, with PFOTES as dispersant.Wherein PFOTES content
For 5wt.%；
Step 3, aluminum phosphate solution step 1 obtained join in the ceramic slurry obtained in step 2, continue ball milling and obtain
To ceramic particle/aluminum phosphate composite ceramics slip, wherein the mass fraction of aluminum phosphate is 30wt%, and ceramic particle content is
40wt%；
Step 4, employing vibration moulding, the composite ceramics slip making step 3 obtain is sufficiently impregnated with quartz fiber cloth, Qi Zhongzhen
Dynamic amplitude 2mm, frequency 15Hz, time of vibration 2min；
Step 5, fiber cloth step 4 obtained successively stack, and use compression molding, and wherein molding pressure is 5MPa,
Obtain composite impregnant；
Step 6, composite impregnant step 5 obtained are placed in drying baker and carry out cured, solidification temperature 120
DEG C, 12h hardening time；
Understanding the composite dielectric constant obtained through above-mentioned steps after tested is 2.8 and the contact angle ≈ of water 140 °,
I.e. obtain moistureproof wave transparent quartz fibre/phosphate ceramics composite.
The above, the only present invention preferably detailed description of the invention, these detailed description of the invention are all based on the present invention
Different implementations under general idea, and protection scope of the present invention is not limited thereto, any are familiar with the art
Technical staff in the technical scope that the invention discloses, the change that can readily occur in or replacement, all should contain the present invention's
Within protection domain.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof, it is characterised in that
Step 1, configuration aluminum phosphate solution: aluminium salt being incorporated in phosphate aqueous solution, arranging bath temperature is 60～100 DEG C, promotees
Entering the dissolving of aluminium salt, and obtain transparent aluminium dihydrogen phosphate aqueous solution, in aluminium dihydrogen phosphate aqueous solution, the quality of aluminium dihydrogen phosphate is divided
Number is 40～80wt.%；
Step 2, configuration containing one or both silicon nitrides, boron nitride, aluminium oxide or the ceramic particle slip of silicon oxide, with ethanol or
Methanol is solvent, with fluorine containing silane as dispersant；Wherein fluorine containing silane is PFTS (C8F13H4SiCl3)、PFOTES
(C14H19F13O3Si), FAS (C8F13H4Si (OCH2CH3) 3) or PTES (C14H19F15O3Si2) therein one or several
Mixing, in ceramic particle slip, the content of silicon fluoride is 0.1～20wt.%；
Step 3, aluminium dihydrogen phosphate aqueous solution step 1 obtained join in the ceramic particle slip obtained in step 2, continue
Ball milling obtains ceramic particle/aluminum phosphate composite ceramics slip, in described ceramic particle/aluminum phosphate composite ceramics slip, and aluminum phosphate
Mass fraction be 20～40wt%, ceramic particle content is 20～50wt%；
Step 4, employing vibration moulding, it is fine that the ceramic particle/aluminum phosphate composite ceramics slip making step 3 obtain is sufficiently impregnated with quartz
Wei Bu, wherein vibration amplitude 2～5mm, frequency 5～100Hz, time of vibration 1～10min；
Step 5, fiber cloth step 4 obtained successively stack, and use compression molding, and wherein molding pressure is 2～10MPa,
Obtain composite impregnant；
Step 6, composite impregnant step 5 obtained are placed in drying baker and carry out cured, solidification temperature 80～200
DEG C, hardening time 12～72h, obtain moistureproof wave transparent quartz fibre/phosphate ceramics composite.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof the most according to claim 1, its feature exists
In, described aluminium salt is aluminium hydroxide or aluminum nitrate.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof the most according to claim 1, its feature exists
In, in described step 1, bath temperature is 85 DEG C.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof the most according to claim 1, its feature exists
In, in described step 4, vibration amplitude 3mm, frequency 56Hz, time of vibration 5min.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof the most according to claim 1, its feature exists
In, in described step 5, molding pressure is 4MPa.
Moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof the most according to claim 1, its feature exists
In, in described step 6, solidification temperature 120 DEG C, 36h hardening time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610584792.0A CN106242550A (en) | 2016-07-22 | 2016-07-22 | A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610584792.0A CN106242550A (en) | 2016-07-22 | 2016-07-22 | A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957179A (en) * | 2017-02-24 | 2017-07-18 | 东华大学 | A kind of SiBN fiber reinforcements SiO2‑BN‑Al2O3The preparation method of wave-penetrating composite material |
| CN109721347A (en) * | 2019-01-14 | 2019-05-07 | 中南大学 | A kind of SiC whisker and C-AlPO4The preparation method of powder modified synergic mullite coating |
| CN113321483A (en) * | 2021-06-03 | 2021-08-31 | 哈尔滨工程大学 | Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material |
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| CN102514346A (en) * | 2011-12-19 | 2012-06-27 | 西南科技大学 | Preparation method of quartz fiber/chrome aluminum phosphate-based high temperature wave-transmitting material |
| CN103664213A (en) * | 2012-09-13 | 2014-03-26 | 南京航空航天大学 | Preparation method of high-temperature wave-transparent composite material toughened by hybrid-woven fibers |
| CN103936390A (en) * | 2014-02-21 | 2014-07-23 | 湖北三江航天江北机械工程有限公司 | Preparation method of phosphate composite material radome body |
| US20150000557A1 (en) * | 2012-01-10 | 2015-01-01 | 3M Innovative Properties Company | Aqueous fluorinated silane dispersions |
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| CN1613824A (en) * | 2004-12-01 | 2005-05-11 | 山东中材先进材料股份有限公司 | Coating material of antenna housing and its preparation |
| CN102514346A (en) * | 2011-12-19 | 2012-06-27 | 西南科技大学 | Preparation method of quartz fiber/chrome aluminum phosphate-based high temperature wave-transmitting material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957179A (en) * | 2017-02-24 | 2017-07-18 | 东华大学 | A kind of SiBN fiber reinforcements SiO2‑BN‑Al2O3The preparation method of wave-penetrating composite material |
| CN106957179B (en) * | 2017-02-24 | 2020-05-29 | 东华大学 | SiBN fiber reinforced SiO2-BN-Al2O3Preparation method of wave-transparent composite material |
| CN109721347A (en) * | 2019-01-14 | 2019-05-07 | 中南大学 | A kind of SiC whisker and C-AlPO4The preparation method of powder modified synergic mullite coating |
| CN109721347B (en) * | 2019-01-14 | 2021-08-24 | 中南大学 | SiC whisker and C-AlPO4Preparation method of powder synergistic modified mullite coating |
| CN113321483A (en) * | 2021-06-03 | 2021-08-31 | 哈尔滨工程大学 | Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material |
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Application publication date: 20161221 |